CN114307636B - Nano photocatalyst air deodorant and preparation method thereof - Google Patents
Nano photocatalyst air deodorant and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nano photocatalyst air deodorant and a preparation method thereof. The nano photocatalyst of the nano photocatalyst air deodorant is prepared by loading tin dioxide on a carbon rubber ball, then loading and preparing titanium dioxide and cerium dioxide and g-C by taking the carbon rubber ball/tin dioxide and graphene oxide as carriers 3 N 4 Mixing and reacting in H 2 And (4) vulcanizing in the S atmosphere to obtain the nano photocatalyst. Compared with the prior art, the nano photocatalyst air deodorant prepared by the nano photocatalyst has the advantages of high visible light catalytic degradation activity and capability of effectively degrading harmful substances such as acetaldehyde and ammonia gas.
Description
Technical Field
The invention relates to the technical field of photocatalysis, in particular to a nano photocatalyst air deodorant and a preparation method thereof.
Background
The air purification aspect is the most important part of the photocatalyst in environmental management, and is mainly divided into indoor and outdoor air cleaning and purification. Especially, the indoor air control has been greatly developed, and the main indoor pollutants are organic substances such as formaldehyde and toluene released from building decoration materials or viruses infected by human respiratory infectious diseases. The existing methods for treating formaldehyde mainly comprise a photocatalysis method, a condensation method, an absorption method, an adsorption method, a biological treatment method and the like. The photocatalytic method is a method of improving the quality of indoor air by decomposing organic substances into carbon monoxide and water using a photocatalyst having an oxidation-reduction ability under a light condition, and can be simply understood as a reverse process of photosynthesis. The photocatalyst is also called as photocatalyst, which is smeared on the surface of a base material or attached to a carrier, generates strong oxidative degradation capability under the action of ultraviolet light and visible light, can effectively degrade toxic and harmful gases, kill various bacteria, and decompose and harmlessly treat toxins released by bacteria or fungi. The core of the photocatalytic reaction is the photocatalyst, and the factors such as the crystalline phase, the particle size, the specific surface area and the like of the photocatalyst have a decisive influence on the photocatalytic oxidation reaction. The existing photocatalysis technology still has great limitation, common photocatalysts cannot fully utilize sunlight due to large particle size and small specific surface area, show strong incompatibility when being combined with most carriers, are very easy to generate condensation phenomenon, even decompose self carriers, cause unsustainability and low efficiency of photocatalysis reaction, mostly can only utilize short-wavelength light of ultraviolet light, have the utilization rate of the sunlight of less than 3 percent, and are difficult to continuously act under normal environmental conditions.
In order to remove indoor air pollutants conveniently and quickly, people have been making efforts on photocatalyst air deodorant. The invention patent with publication number CN106362584A discloses a nano photocatalyst air deodorant and a preparation method thereof, and the nano photocatalyst air deodorant consists of the following materials in parts by weight: 2 to 8 percent of nano titanium dioxide, 1 to 5 percent of active agent, 2 to 6 percent of nano silver powder, 2 to 5 percent of negative ion powder, 1 to 5 percent of dispersant, 1 to 5 percent of penetrating agent, 0.5 to 3 percent of wave absorbing factor (wave absorbing agent) and 70 to 85 percent of deionized water. The prepared nano photocatalyst air deodorant can actively capture organic pollutants under the condition of visible light or natural light, directly decompose harmful gases such as formaldehyde and the like, and convert the harmful gases into carbon dioxide and water. The nano titanium dioxide has high ultraviolet light catalysis efficiency, but has low solar light absorption rate, and although the wave absorbing agent is added, the effect of removing organic matters in the air under visible light is still not good.
The invention patent with publication number CN109569288A discloses a photocatalyst deodorant and a preparation method thereof, which is prepared by the following materials in parts by weight: 5-10 parts of nano titanium dioxide, 1-3 parts of anion powder, 1-2 parts of indium phosphate, 1-5 parts of a penetrating agent, 1-5 parts of a dispersing agent, 5-10 parts of sodium bicarbonate, 70-90 parts of deionized water, 3-5 parts of aloe vera gel and 10-15 parts of tea polyphenol.
The invention patent with publication number CN107899591A discloses a photocatalyst sterilization air cleaner and a preparation method thereof, and the photocatalyst sterilization air cleaner comprises SnS 2 Nanosheet and TiO 2 Nanoparticles, tiO 2 The nano particles are compounded in SnS 2 Surface of nanosheet, tiO 2 Nanoparticles in SnS 2 The surfaces of the nano sheets are in punctate intensive distribution, and the obtained photocatalyst sterilizing air cleaner has good appearance, simple operation, high yield and low preparation cost. SnS 2 Improve TiO 2 Low utilization rate of sunlight, but TiO 2 Nanoparticles and SnS 2 The binding force of the nano sheets is not firm, and the nano sheets are distributed in a dotted manner but are not uniformly distributed, so that the effect of the photocatalyst sterilization air cleaning agent can be directly influenced.
Disclosure of Invention
In view of the problems of poor sunlight absorption and utilization rate and insignificant effect of the photocatalyst scavenger in the prior art, the technical problem to be solved by the invention is to provide a photocatalyst air scavenger which can efficiently utilize sunlight energy and has high catalytic degradation activity on organic gas.
In order to achieve the aim, the invention provides a preparation method of a nano photocatalyst air deodorant, which comprises the following steps of:
step 1, dissolving 0.3-0.6 part of vegetable gum in 50-80 parts of water, adding 5-15 parts of nano photocatalyst, 2-6 parts of ceramsite sand, 3-10 parts of vegetable extract and 1-3 parts of adhesive auxiliary agent, and stirring for 30-60 minutes at 500-800 revolutions per minute to obtain a coating dispersion mixture;
and 2, immersing the activated carbon fibers into the coating dispersion mixture prepared in the step 1, stirring for 10-30 minutes at 200-400 revolutions per minute, and drying for 5-8 hours at the temperature of 45-80 ℃ to obtain the nano photocatalyst air deodorant.
Preferably, the vegetable gum in the step 1 is one of guar gum, fenugreek gum and sesbania gum.
Preferably, the preparation method of the nano photocatalyst in step 1 is as follows:
s1, dissolving sucrose in water, and adding SnCl 4 ·5H 2 O, stirring and mixing uniformly, adjusting the pH value of the mixed solution to 11-13, continuously stirring for 10-30 minutes, transferring to a reaction kettle for hydrothermal reaction, naturally cooling, centrifugally collecting solids, washing and drying to obtain carbon rubber balls/tin dioxide;
s2, adding tetrabutyl titanate and carbon rubber sphere/tin dioxide into absolute ethyl alcohol, and stirring and mixing uniformly after ultrasonic dispersion to obtain a dispersion solution; adding tetrabutyl titanate ethanol solution into the dispersion solution, and stirring and mixing uniformly to obtain solution A; then, mixing absolute ethyl alcohol, water, acetic acid, cerous nitrate hexahydrate and graphene oxide, performing ultrasonic dispersion, and stirring and mixing uniformly to obtain a solution B; dropwise adding the solution B into the solution A, stirring for 4-8 hours, transferring the solution B into a reaction kettle for hydrothermal reaction, cooling, centrifuging, collecting solids, washing, drying, and calcining at 650-700 ℃ for 2-4 hours to obtain a nano photocatalyst A;
s3, mixing g-C 3 N 4 Mixing with nano photocatalyst A, grinding, and introducing H 2 S gas in H 2 And (3) vulcanizing for 10-16 h under the S atmosphere, and cooling to room temperature to obtain the nano photocatalyst.
Further preferably, the preparation method of the nano photocatalyst in the step 1 is as follows, wherein the parts are all parts by weight:
s1, dissolving 20-40 parts of cane sugar in 140-180 parts of water, and adding 2.4-7.4 parts of SnCl 4 ·5H 2 O, stirring for 10-20 minutes at 300-600 revolutions per minute to obtain a mixed solution; adding 0.5-1.2 mol/L sodium hydroxide aqueous solution to adjust the pH of the mixed solution to 11-13, continuously stirring for 10-30 minutes at 300-600 revolutions/minute, carrying out hydrothermal reaction for 6-10 hours at 140-200 ℃ in a reaction kettle, naturally cooling to 20-30 ℃, centrifugally collecting solids at 5000-10000 revolutions/minute, respectively washing for 2-4 times by using absolute ethyl alcohol and water, drying for 3-6 hours at 60-90 ℃ to obtain the carbon rubber ball/dioxideTin;
s2, putting 4.5-10.5 parts of tetrabutyl titanate and 1.8-4.2 parts of the carbon glue balls/tin dioxide prepared in the step S1 into 20-40 parts of absolute ethyl alcohol, performing ultrasonic dispersion for 10-20 minutes, and stirring at 400-600 rpm for 45-90 minutes to obtain a dispersion solution; adding 10-20 parts of tetrabutyl titanate ethanol solution with the concentration of 40-60 mg/L into the dispersion solution, and stirring for 45-90 minutes at 400-600 revolutions/minute to obtain solution A; then 5-15 parts of absolute ethyl alcohol, 2-8 parts of water, 10-20 parts of acetic acid, 0.2-0.5 part of cerous nitrate hexahydrate and 0.03-0.08 part of graphene oxide are mixed, subjected to ultrasonic treatment for 2-5 minutes, and stirred at 400-600 rpm for 45-90 minutes to obtain a solution B; dropwise adding the solution B into the solution A, stirring for 4-8 hours at 400-600 revolutions per minute, reacting for 20-28 hours at 110-150 ℃ in a reaction kettle, cooling to 20-30 ℃, centrifugally collecting solids at 5000-10000 revolutions per minute, respectively cleaning for 2-4 times by using absolute ethyl alcohol and water, carrying out vacuum drying for 6-10 hours at 60-90 ℃, calcining for 2-4 hours at 650-700 ℃, and raising the temperature at the rate of 3-6 ℃/minute to obtain a nano photocatalyst A;
s3, mixing g-C 3 N 4 And the nano photocatalyst A prepared in the step S2 is added with the nano photocatalyst A in a mass ratio of 1: (3-7), grinding for 10-30 minutes at 200-400 r/min, and introducing H at 15-25 mL/s 2 S gas at H 2 And (3) vulcanizing at 175-185 ℃ for 10-16 hours in the S atmosphere, cooling at the speed of 10 ℃/minute to 20-30 ℃ to obtain the nano photocatalyst.
Preferably, the ultrasound parameters in step S2 are: the ultrasonic parameters are as follows: 2800-3200W and 18000-22000 Hz.
Preferably, the grain size of the ceramsite sand in the step 1 is 30-70 meshes.
Preferably, in the step 1, the plant extract is gardenia essential oil and honeysuckle extract according to a weight ratio of 1: (3-10) mixing the components.
Preferably, the adhesion promoter in the step 1 is a mixture of polyethylene glycol and silica sol in a weight ratio of 1 (2-4).
Preferably, the activated carbon fiber in the step 2 is one of an activated carbon fiber plate and an activated carbon fiber ball, the sizes of the activated carbon fiber plate and the activated carbon fiber ball are respectively (10-30) cm x (10-30) cm, and the diameter of the activated carbon fiber plate and the activated carbon fiber ball is 10-15 cm.
The nano photocatalyst air deodorant utilizes a nano photocatalyst in the deodorant to catalytically degrade toxic and harmful substances in the air under the irradiation of solar light energy so as to achieve the effect of removing the smell. According to the invention, a heterojunction hollow nano photocatalyst is used as a main action component of the deodorant, ceramsite and plant extract are added, the nano photocatalyst is coated on active carbon fibers through plant glue and adhesive, and the nano photocatalyst is dried to obtain the nano photocatalyst air deodorant. The ceramic grain sand adsorbs part of the heterojunction hollow nano photocatalyst, disperses the heterojunction hollow nano photocatalyst on the active carbon fiber and provides more space for gas circulation; the coating dispersion mixture uses the vegetable gum as a main matrix, and because the vegetable gum can generate a mildewing condition in use, the vegetable extract is added to inhibit the mildewing of the vegetable gum, and the vegetable extract contains vegetable aromatic substances, so that the coated nano photocatalyst air deodorant has vegetable aroma; the mixture of polyethylene glycol and silica sol is used as an adhesive auxiliary agent for coating and dispersing the mixture, the adhesive effect of the adhesive is obviously greater than that of single polyethylene glycol and silica sol, and the adhesive effect of the nano photocatalyst on the activated carbon fiber is improved.
The nano photocatalyst is used as a photocatalyst material in the nano photocatalyst air deodorant and is prepared by hydrolyzing sucrose and SnCl 4 ·5H 2 O, generating monosaccharide and tin hydroxide, preparing carbon gel balls/tin dioxide through a hydrothermal reaction, adding a titanium source, graphene oxide and cerous nitrate hexahydrate, performing an ultrasonic treatment, and then performing a hydrothermal reaction to synthesize titanium dioxide and cerium dioxide to obtain a nano photocatalyst A; finally, the nano-photocatalyst A and g-C are added 3 N 4 Mixing in H 2 And (3) vulcanizing at 175-185 ℃ in the S atmosphere, and then cooling at 10 ℃/min to obtain the nano photocatalyst. After the graphene oxide is subjected to ultrasonic dispersion, the graphene oxide is combined with carbon gel spheres/tin dioxide in a hydrothermal reaction to serve as a reaction carrier, the carbon gel spheres with hydroxyl groups on the surfaces adsorb cationic titanium ions and cerium ions, so that nano titanium dioxide and nano cerium dioxide which are uniformly distributed are generated on the carrier in situ to obtain a nano photocatalyst A, the graphene oxide promotes the generation of hydroxyl radicals on the surfaces of materials, and the carbon gel spheres are calcined to serve as a reaction carrierThe hollow structure formed by burning improves the concentrated absorption of light and is beneficial to carrying out photocatalytic reaction; the nano titanium dioxide and the cerium dioxide are used as photocatalytic materials, the nano titanium dioxide has excellent performance of catalytically degrading harmful gases under ultraviolet illumination, but the nano titanium dioxide is not good in absorption and utilization of visible light under solar illumination, the cerium dioxide has certain sunlight catalytic degradation performance but low degradation efficiency, and the tin dioxide has good photocatalytic performance under the visible light illumination, so that the utilization condition of the photocatalyst material on the sunlight energy is improved. Nano-photocatalyst A and g-C 3 N 4 Mixing, sulfurizing with hydrogen sulfide at high temperature to obtain stannic oxide and cerium disulfide, graphene oxide and g-C 3 N 4 Due to the stack of pi-pi bonds, the light utilization rate and the photooxidation capacity of the material are improved, and simultaneously g-C 3 N 4 The material and titanium dioxide, tin sulfide and cerium sulfide form a heterojunction, so that electron hole pairs generated after the material is irradiated by light can be quickly and effectively separated, the hole is transferred to the surface of the material and reacts with hydroxyl groups on the surface of the material to generate hydroxyl free radicals, organic matters are oxidatively decomposed, and the photocatalytic activity is improved. After the stannic oxide and the cerium dioxide are vulcanized, the cerium disulfide, the stannic disulfide and the titanium dioxide generate charge transfer synergistic effect on different interfaces, so that a large number of electrons and holes are generated on the photocatalytic surface, and the catalytic activity is improved.
Based on the technical scheme, compared with the prior art, the nano photocatalyst air deodorant has the advantages that: 1) The carbon rubber ball is used for loading the tin disulfide, the cerium disulfide and the titanium dioxide, the problem that the titanium dioxide is not good in visible light utilization is solved, the visible light utilization rate is increased, excellent photocatalytic activity is achieved under the visible light, and the degradation efficiency of organic air pollutants is improved. 2) Graphene oxide and g-C 3 N 4 Stacking, increasing the photocatalytic activity of the material, while g-C 3 N 4 And the material forms a heterojunction with tin disulfide, cerium disulfide and titanium dioxide, so that electron hole pairs are rapidly separated to generate hydroxyl radicals, and the photocatalytic degradation performance of the material is improved.
Detailed Description
The raw material sources used in the examples and comparative examples are as follows:
guar gum: biological engineering ltd, shandong changxiao, CAS number: 9000-30-3, main effective components: guar gum, active substance content: 99%, cargo number: 101.
ceramsite sand: zhengzhou jiuqin refractory limited, density: 1.65g/cm 3 And the goods number: 025, particle size: 30-70 meshes, 30-50% of porosity and adsorption rate: 80 to 90 percent.
Gardenia essential oil: wanxiangxiang flavor Co, jiangxi.
Honeysuckle extract: huzhou Zhenlu biological products, inc.
Silica sol: guangdong Hui and silicon products, model number: s-1430, viscosity at 25 ℃ is less than or equal to 6.5 Pa.s, silicon dioxide content: 29 to 31 percent.
An activated carbon fiber plate: jiangsu Sensen carbon science and technology Co., ltd, mesh: 200 meshes.
SnCl 4 ·5H 2 O: shanghai mairei chemical technology ltd, CAS No.: 1026-06-9.
Tetrabutyl titanate: wuxi, citizen, yatai Union chemical Co., ltd, CAS number: 5593-70-4.
Cerous nitrate hexahydrate: shandongsheng New materials, inc., CAS number: 10294-41-4.
And (3) graphene oxide: hangzhou intelligent titanium purification science and technology source manufacturer, average thickness: 1-3 nm, layer number: 2-5 layers, carbon content: 99wt%, specific surface area: 20 to 50m 2 /g。
g-C 3 N 4 : kuntongjiang chemical reagents ltd, CAS no: 143334-20-7, purity: 99 percent.
Example 1
A preparation method of a nano photocatalyst air deodorant comprises the following steps:
step 1, dissolving 0.4g of guar gum in 65g of water, adding 10g of nano photocatalyst, 4g of ceramsite sand, 6g of plant extract of gardenia essential oil and honeysuckle extract mixed according to a weight ratio of 1;
and 2, immersing an activated carbon fiber plate with the size of 20cm multiplied by 20cm into the coating dispersion mixture prepared in the step 1, stirring for 20 minutes at 300 revolutions per minute, and drying for 6.5 hours at the temperature of 60 ℃ to obtain the nano photocatalyst air deodorant.
The preparation method of the nano photocatalyst in the step 1 comprises the following steps:
s1, dissolving 30g of sucrose in 160g of water, and adding 4.2g of SnCl 4 ·5H 2 O, stirring for 15 minutes at the speed of 400 revolutions per minute to obtain a mixed solution; adding a sodium hydroxide aqueous solution with the concentration of 1mol/L to adjust the pH value of the mixed solution to 12, continuously stirring at 500 r/min for 20 minutes, carrying out hydrothermal reaction at 180 ℃ in a reaction kettle for 8 hours, naturally cooling to 25 ℃, centrifuging at 7000 r/min to collect solids, respectively washing with absolute ethyl alcohol and water for 3 times, and drying at 80 ℃ for 5 hours to obtain carbon rubber balls/tin dioxide;
s2, placing 7.5g of tetrabutyl titanate and 3g of the carbon colloidal spheres/tin dioxide prepared in the step S1 into 30g of absolute ethyl alcohol, and carrying out ultrasonic dispersion for 15 minutes, wherein the ultrasonic parameters are as follows: stirring at 3000W and 20000 Hz at 500 rpm for 60 min to obtain dispersion solution; adding 15g of tetrabutyl titanate ethanol solution with the concentration of 50mg/L into the dispersion solution, and stirring for 60 minutes at 500 revolutions per minute to obtain solution A; then 10g of absolute ethyl alcohol, 6g of water, 15g of acetic acid, 0.36g of cerous nitrate hexahydrate and 0.05g of graphene oxide are mixed, and subjected to ultrasonic treatment for 3 minutes, wherein the ultrasonic parameters are as follows: stirring at 3000W and 20000 Hz for 60 min at 500 rpm to obtain solution B; adding the solution B into the solution A at a speed of 3 drops/second, stirring for 6 hours at 500 revolutions/minute, reacting for 24 hours at 135 ℃ in a reaction kettle, cooling to 25 ℃, centrifuging at 7000 revolutions/minute, collecting solids, washing for 3 times respectively by using absolute ethyl alcohol and water, vacuum drying for 8 hours at 85 ℃, calcining for 3 hours at 680 ℃, and heating at a speed of 5 ℃/minute to obtain a nano photocatalyst A;
s3, mixing 1 g-C 3 N 4 Mixing with 4g of the nano photocatalyst A prepared in the step S2, grinding for 20 minutes at 300 revolutions per minute, and introducing H at 20mL per second 2 S gas at H 2 Sulfuration is carried out for 14 hours at 180 ℃ under the S atmosphere, then the temperature is reduced at the speed of 10 ℃/minute,and cooling to 25 ℃ to obtain the nano photocatalyst.
Example 2
A method for preparing a nano photocatalyst air deodorant, which is basically the same as that in example 1, and only differs from the following steps: the preparation methods of the nano photocatalyst in the step 1 are inconsistent.
The preparation method of the nano photocatalyst in the step 1 comprises the following steps:
s1, adding 4.2g SnCl into 160g of water 4 ·5H 2 O, stirring for 15 minutes at the speed of 400 revolutions per minute to obtain a mixed solution; adding a sodium hydroxide aqueous solution with the concentration of 1mol/L to adjust the pH value of the mixed solution to 12, continuously stirring at 500 r/min for 20 minutes, carrying out hydrothermal reaction at 180 ℃ in a reaction kettle for 8 hours, naturally cooling to 25 ℃, centrifuging at 7000 r/min to collect solids, respectively washing with absolute ethyl alcohol and water for 3 times, and drying at 80 ℃ for 5 hours to obtain tin dioxide;
s2, placing 7.5g of tetrabutyl titanate and 3g of the tin dioxide prepared in the step S1 into 30g of absolute ethyl alcohol, and ultrasonically dispersing for 15 minutes, wherein the ultrasonic parameters are as follows: stirring at 3000W and 20000 Hz at 500 rpm for 60 min to obtain dispersion solution; adding 15g of tetrabutyl titanate ethanol solution with the concentration of 50mg/L into the dispersion solution, and stirring for 60 minutes at 500 revolutions per minute to obtain solution A; then 10g of absolute ethyl alcohol, 6g of water, 15g of acetic acid, 0.36g of cerous nitrate hexahydrate and 0.05g of graphene oxide are mixed, and subjected to ultrasonic treatment for 3 minutes, wherein the ultrasonic parameters are as follows: stirring at 3000W and 20000 Hz for 60 min at 500 rpm to obtain solution B; adding the solution B into the solution A at a speed of 3 drops/second, stirring for 6 hours at 500 revolutions/minute, reacting for 24 hours at 135 ℃ in a reaction kettle, cooling to 25 ℃, centrifuging at 7000 revolutions/minute, collecting solids, washing for 3 times respectively by using absolute ethyl alcohol and water, vacuum drying for 8 hours at 85 ℃, calcining for 3 hours at 680 ℃, and heating at a rate of 5 ℃/minute to obtain a nano photocatalyst A;
s3, mixing 1 g-C 3 N 4 Mixing with 4g of the nano photocatalyst A prepared in the step S2, grinding for 20 minutes at 300 revolutions per minute, and introducing H at 20mL/S 2 S gas in H 2 And (3) vulcanizing at 180 ℃ for 14 hours under the S atmosphere, cooling at the speed of 10 ℃/minute, and cooling to 25 ℃ to obtain the nano photocatalyst.
Example 3
A method for preparing a nano photocatalyst air deodorant, which is basically the same as that in example 1, and only differs from the following steps: the preparation method of the nano photocatalyst in the step 1 is inconsistent.
The preparation method of the nano photocatalyst in the step 1 comprises the following steps:
s1, dissolving 30g of sucrose in 160g of water, and stirring for 15 minutes at 400 revolutions per minute to obtain a mixed solution; adding a sodium hydroxide aqueous solution with the concentration of 1mol/L to adjust the pH value of the mixed solution to 12, continuously stirring at 500 r/min for 20 minutes, carrying out hydrothermal reaction at 180 ℃ for 8 hours in a reaction kettle, naturally cooling to 25 ℃, centrifuging at 7000 r/min to collect solids, respectively washing with absolute ethyl alcohol and water for 3 times, and drying at 80 ℃ for 5 hours to obtain carbon rubber balls;
s2, placing 7.5g of tetrabutyl titanate and 3g of the carbon rubber spheres prepared in the step S1 into 30g of absolute ethyl alcohol, and carrying out ultrasonic dispersion for 15 minutes, wherein the ultrasonic parameters are as follows: stirring at 3000W and 20000 Hz at 500 rpm for 60 min to obtain dispersion solution; adding 15g of tetrabutyl titanate ethanol solution with the concentration of 50mg/L into the dispersion solution, and stirring for 60 minutes at 500 revolutions per minute to obtain solution A; then 10g of absolute ethyl alcohol, 6g of water, 15g of acetic acid, 0.36g of cerous nitrate hexahydrate and 0.05g of graphene oxide are mixed, and subjected to ultrasonic treatment for 3 minutes, wherein the ultrasonic parameters are as follows: stirring at 3000W and 20000 Hz at 500 rpm for 60 min to obtain solution B; adding the solution B into the solution A at a speed of 3 drops/second, stirring for 6 hours at 500 revolutions/minute, reacting for 24 hours at 135 ℃ in a reaction kettle, cooling to 25 ℃, centrifuging at 7000 revolutions/minute, collecting solids, washing with absolute ethyl alcohol and water for 3 times, drying under vacuum at 85 ℃ for 8 hours, calcining at 680 ℃ for 3 hours at a temperature rise rate of 5 ℃/minute, and obtaining the nano photocatalyst A;
s3, mixing 1g of C 3 N 4 Mixing with 4g of the nano photocatalyst A prepared in the step S2, grinding for 20 minutes at 300 revolutions per minute, and introducing H at 20mL/S 2 S gas at H 2 And (3) vulcanizing at 180 ℃ for 14 hours under the S atmosphere, cooling at the speed of 10 ℃/minute, and cooling to 25 ℃ to obtain the nano photocatalyst.
Example 4
A method for preparing a nano photocatalyst air deodorant, which is basically the same as the method in the example 1, and only differs from the method in that: the preparation method of the nano photocatalyst in the step 1 is inconsistent.
The preparation method of the nano photocatalyst in the step 1 comprises the following steps:
s1, dissolving 30g of sucrose in 160g of water, and adding 4.2g of SnCl 4 ·5H 2 O, stirring for 15 minutes at the speed of 400 revolutions per minute to obtain a mixed solution; adding a sodium hydroxide aqueous solution with the concentration of 1mol/L to adjust the pH value of the mixed solution to 12, continuously stirring at 500 r/min for 20 minutes, carrying out hydrothermal reaction at 180 ℃ for 8 hours in a reaction kettle, naturally cooling to 25 ℃, centrifuging at 7000 r/min to collect solids, respectively washing with absolute ethyl alcohol and water for 3 times, and drying at 80 ℃ for 5 hours to obtain carbon rubber balls/tin dioxide;
s2, placing 7.5g of tetrabutyl titanate and 3g of the carbon colloidal spheres/tin dioxide prepared in the step S1 into 30g of absolute ethyl alcohol, and carrying out ultrasonic dispersion for 15 minutes, wherein the ultrasonic parameters are as follows: stirring at 3000W and 20000 Hz at 500 rpm for 60 min to obtain dispersion solution; adding 15g of tetrabutyl titanate ethanol solution with the concentration of 50mg/L into the dispersion solution, and stirring for 60 minutes at 500 revolutions per minute to obtain solution A; then 10g of absolute ethyl alcohol, 6g of water, 15g of acetic acid and 0.36g of cerous nitrate hexahydrate are subjected to ultrasonic treatment for 3 minutes, wherein ultrasonic parameters are as follows: stirring at 3000W and 20000 Hz for 60 min at 500 rpm to obtain solution B; adding the solution B into the solution A at a speed of 3 drops/second, stirring for 6 hours at 500 revolutions/minute, reacting for 24 hours at 135 ℃ in a reaction kettle, cooling to 25 ℃, centrifuging at 7000 revolutions/minute, collecting solids, washing with absolute ethyl alcohol and water respectively for 3 times, vacuum drying at 85 ℃ for 8 hours, calcining at 680 ℃ for 3 hours at a temperature rise rate of 5 ℃/minute, and obtaining the nano photocatalyst A;
s3, mixing 1 g-C 3 N 4 Mixing with 4g of the nano photocatalyst A prepared in the step S2, grinding for 20 minutes at 300 revolutions per minute, and introducing H at 20mL/S 2 S gas at H 2 And (3) vulcanizing at 180 ℃ for 14 hours under the S atmosphere, cooling at the speed of 10 ℃/minute, and cooling to 25 ℃ to obtain the nano photocatalyst.
Example 5
A method for preparing a nano photocatalyst air deodorant, which is basically the same as that in example 1, and only differs from the following steps: the preparation methods of the nano photocatalyst in the step 1 are inconsistent.
The preparation method of the nano photocatalyst in the step 1 comprises the following steps:
s1, dissolving 30g of sucrose in 160g of water, and adding 4.2g of SnCl 4 ·5H 2 O, stirring for 15 minutes at the speed of 400 revolutions per minute to obtain a mixed solution; adding a sodium hydroxide aqueous solution with the concentration of 1mol/L to adjust the pH value of the mixed solution to 12, continuously stirring at 500 r/min for 20 minutes, carrying out hydrothermal reaction at 180 ℃ for 8 hours in a reaction kettle, naturally cooling to 25 ℃, centrifuging at 7000 r/min to collect solids, respectively washing with absolute ethyl alcohol and water for 3 times, and drying at 80 ℃ for 5 hours to obtain carbon rubber balls/tin dioxide;
s2, placing 7.5g of tetrabutyl titanate and 3g of the carbon colloidal spheres/tin dioxide prepared in the step S1 into 30g of absolute ethyl alcohol, and carrying out ultrasonic dispersion for 15 minutes, wherein the ultrasonic parameters are as follows: stirring at 3000W and 20000 Hz at 500 rpm for 60 min to obtain dispersion solution; adding 15g of tetrabutyl titanate ethanol solution with the concentration of 50mg/L into the dispersion solution, and stirring for 60 minutes at 500 revolutions per minute to obtain solution A; then 10g of absolute ethyl alcohol, 6g of water, 15g of acetic acid, 0.36g of cerous nitrate hexahydrate and 0.05g of graphene oxide are mixed, and subjected to ultrasonic treatment for 3 minutes, wherein the ultrasonic parameters are as follows: stirring at 3000W and 20000 Hz at 500 rpm for 60 min to obtain solution B; adding the solution B into the solution A at a speed of 3 drops/second, stirring for 6 hours at 500 revolutions/minute, reacting for 24 hours at 135 ℃ in a reaction kettle, cooling to 25 ℃, centrifuging at 7000 revolutions/minute, collecting solids, washing with absolute ethyl alcohol and water for 3 times, drying under vacuum at 85 ℃ for 8 hours, calcining at 680 ℃ for 3 hours at a temperature rise rate of 5 ℃/minute, and obtaining the nano photocatalyst A;
s3, grinding the nano photocatalyst A prepared in the step S2 at 300 revolutions per minute for 20 minutes, and introducing H at 20mL/S 2 S gas in H 2 And (3) vulcanizing at 180 ℃ for 14 hours under the S atmosphere, cooling at the speed of 10 ℃/minute, and cooling to 25 ℃ to obtain the nano photocatalyst.
Comparative example 1
A method for preparing a nano photocatalyst air deodorant, which is basically the same as that in example 1, and only differs from the following steps: the preparation methods of the nano photocatalyst in the step 1 are inconsistent.
The preparation method of the nano photocatalyst in the step 1 comprises the following steps:
s1, placing 7.5g of tetrabutyl titanate into 30g of absolute ethyl alcohol, and ultrasonically dispersing for 15 minutes, wherein ultrasonic parameters are as follows: stirring at 3000W and 20000 Hz at 500 rpm for 60 min to obtain dispersion solution; adding 15g of tetrabutyl titanate ethanol solution with the concentration of 50mg/L into the dispersion solution, and stirring for 60 minutes at 500 revolutions per minute to obtain solution A; then 10g of absolute ethyl alcohol, 6g of water, 15g of acetic acid and 0.36g of cerous nitrate hexahydrate are mixed and subjected to ultrasonic treatment for 3 minutes, wherein the ultrasonic parameters are as follows: stirring at 3000W and 20000 Hz for 60 min at 500 rpm to obtain solution B; adding the solution B into the solution A at a speed of 3 drops/second, stirring for 6 hours at 500 revolutions/minute, reacting for 24 hours at 135 ℃ in a reaction kettle, cooling to 25 ℃, centrifuging at 7000 revolutions/minute, collecting solids, washing with absolute ethyl alcohol and water respectively for 3 times, vacuum drying at 85 ℃ for 8 hours, calcining at 680 ℃ for 3 hours at a temperature rise rate of 5 ℃/minute, and obtaining the nano photocatalyst A;
s2, grinding the nano photocatalyst A prepared in the step S1 at 300 revolutions per minute for 20 minutes, and introducing H at 20mL/S 2 S gas in H 2 And (3) vulcanizing at 180 ℃ for 14 hours under the S atmosphere, cooling at the speed of 10 ℃/minute, and cooling to 25 ℃ to obtain the nano photocatalyst.
Comparative example 2
A method for preparing a nano photocatalyst air deodorant, which is basically the same as that in example 1, and only differs from the following steps: no nano photocatalyst is added in the step 1.
Test example 1
Formaldehyde and acetaldehyde purification test:
according to the national standard GB/T23761-2020 < test method for acetaldehyde (or formaldehyde) of photocatalytic material and product air purification performance test method for degrading acetaldehyde >:
1. cutting the photocatalyst air deodorant into a flaky sample with the length (99.5 +/-0.5) mm, the width (49.5 +/-0.5) mm and the thickness of 5 mm;
2. introducing acetaldehyde into the photocatalytic reactor, regulating acetaldehyde flow to (1 + -0.02) L/min, and controlling acetaldehyde concentration to (1 + -0.05) mL/m 3 Starting and calibrating a gas chromatograph, measuring the concentration of acetaldehyde in the reaction gas, continuously measuring for three times, and averaging to obtain the initial concentration (phi) of acetaldehyde in the reaction gas A0 )；
3. Drying and ultraviolet irradiating the flaky sample in a pollution-free gas environment, placing the flaky sample on a photocatalytic reactor adjusting block, and adjusting the height of the adjusting block to ensure that the average value of the visible light irradiation of the surface of the flaky sample is (30 +/-0.5) mW/cm 2 ；
4. Under the condition of not turning on a light source, the reactor is fed with the solution with the concentration of 1mL/m at the speed of 2mL/s 3 Measuring the concentration of carbon dioxide at the outlet, when the concentration of carbon dioxide at the outlet (phi) B0 ) Is stable and less than 1mL/m 3 Then, the acetaldehyde introduction process of the step 2 is carried out, the acetaldehyde concentration at the outlet of the catalytic reactor is measured, and when the acetaldehyde concentration at the outlet is stable (the concentration is not lower than phi) A0 90%) of acetaldehyde, as the initial concentration of acetaldehyde for the photocatalytic reaction (. Phi.)) Ap0 )；
5. Continuously introducing acetaldehyde, starting visible light (fluorescent lamp with color temperature of 5000K), testing outlet acetaldehyde concentration and carbon dioxide concentration every 15min, reacting for 5 hours, and taking the average value of 3 acetaldehyde concentrations and carbon dioxide concentrations obtained at the end of the reaction as the acetaldehyde concentration (phi) after visible light catalytic reaction Apn ) And carbon dioxide concentration (phi) Bn )；
6. Acetaldehyde photocatalytic removal rate P r ＝(φ Ap0 -φ Apn )/φ Ap0 ×100％；
7. Acetaldehyde mineralization rate M Ar ＝(φ Bn -φ B0 )/((φ Ap0 -φ Apn )×2)×100％；
8. Photocatalytic removal rate (P) of formaldehyde CF ) Obtained by conversion of acetaldehyde photocatalytic removal rate and used for representing formaldehyde removal rate, P CF ＝P r 。
The test results are shown in Table 1.
Test example 2
And (3) purified ammonia gas test:
according to journal papers (research on the degradation effect of the loaded titanium dioxide P25 photocatalyst on ammonia gas, author: betula futokadsense et al, university of Sichuan agriculture, 2016, 9 months), a photocatalytic degradation test is performed on ammonia gas by using the photocatalyst air deodorant, and the test process is as follows:
1. cutting the photocatalyst air deodorant into a flaky sample with the diameter of 5cm and the thickness of 0.5 cm;
2. placing a sheet sample in a photocatalytic reactor, setting the relative humidity to be 75 percent and the temperature to be 13 ℃, not starting a light source, introducing ammonia gas with the initial concentration of 120-130 mg/L/with the flow rate of 200L/h, detecting the concentration of the outlet ammonia gas every 10min until the concentration of the outlet ammonia gas reaches the balanced stable state, and taking the stable concentration as the initial concentration (phi) of the ammonia gas of the photocatalytic reaction NH30 )；
3. Continuously introducing ammonia gas, starting a light source (the light source selects a fluorescent lamp with the color temperature of 5000K), testing the concentration of acetaldehyde and the concentration of carbon dioxide at an outlet every 15min, reacting for 5 hours, and taking the average value of 3 ammonia gas concentrations obtained at the end of the reaction as the concentration (phi) of the ammonia gas after the photocatalytic reaction NH3n )；
4. Ammonia photocatalytic removal rate = P NH3 (φ NH30 -φ NH3n )/φ NH30 ×100％。
The test results are shown in Table 1.
TABLE 1 photocatalyst air odor removal agent decontamination test results
The comparison of the example 1 with the examples 2-5 and the comparative examples 1-2 shows that the visible light catalytic removal rate of the acetaldehyde, the formaldehyde and the ammonia gas is the best in the example 1, and probably, the sucrose and the SnCl 4 ·5H 2 Carrying out hydrothermal load on O to generate carbon gel balls/tin dioxide, improving the specific surface area of the material, providing active sites for photocatalytic reaction, and simultaneously enhancing the activity of visible catalytic reaction by the tin dioxide; carbon rubber ball and oxidized stoneThe graphene is used as a carrier, and the carbon rubber spheres are loaded on the surface of the graphene oxide sheet layer, so that the specific surface area is increased, the hollow structure of the carbon rubber spheres improves the concentrated absorption of light, promotes the generation of hydroxyl radicals on the surface of the graphene oxide, and improves the photocatalytic degradation efficiency; functional groups on the surface of the carbon colloidal spheres have group coordination with cerium ions and titanium ions, and the adsorbed cerium ions and titanium ions reach the surface of the carbon colloidal spheres and are converted into cerium dioxide and titanium dioxide, so that the condition of low visible light utilization rate of the titanium dioxide is improved, and the visible light catalytic effect of the material is improved; the stannic oxide and cerium dioxide are vulcanized to generate stannic disulfide and cerium disulfide, and the photocatalysis effect is enhanced; in the vulcanization process, graphene oxide and g-C 3 N 4 Stacking through pi-pi bonds to form a spatial laminated structure with hollow carbon rubber spheres loaded on graphene oxide, and simultaneously g-C 3 N 4 And the active sites of hydroxyl radicals are increased, the absorption of light energy is improved, and the visible light catalytic degradation efficiency is effectively enhanced.
Claims (9)
1. A preparation method of a nano photocatalyst air deodorant is characterized by comprising the following steps:
dissolving plant gum in water, adding a nano photocatalyst, ceramsite sand, plant extract and an adhesive auxiliary agent, and stirring to obtain a coating dispersion mixture;
step 2, immersing the activated carbon fibers into the coating dispersion mixture prepared in the step 1, stirring and drying to obtain the nano photocatalyst air deodorant;
the preparation method of the nano photocatalyst in the step 1 comprises the following steps:
s1, dissolving sucrose in water, and adding SnCl 4 ·5H 2 O, stirring and mixing uniformly, adjusting the pH value of the mixed solution to 11-13, continuously stirring for 10-30 minutes, transferring to a reaction kettle for hydrothermal reaction, naturally cooling, centrifugally collecting solids, washing and drying to obtain carbon rubber balls/tin dioxide;
s2, adding tetrabutyl titanate and carbon rubber sphere/tin dioxide into absolute ethyl alcohol, and stirring and mixing uniformly after ultrasonic dispersion to obtain a dispersion solution; adding tetrabutyl titanate ethanol solution into the dispersion solution, and stirring and mixing uniformly to obtain solution A; then, mixing absolute ethyl alcohol, water, acetic acid, cerous nitrate hexahydrate and graphene oxide, performing ultrasonic dispersion, and stirring and mixing uniformly to obtain a solution B; dropwise adding the solution B into the solution A, stirring for 4-8 hours, transferring the solution B into a reaction kettle for hydrothermal reaction, cooling, centrifuging, collecting solids, washing, drying, and calcining at 650-700 ℃ for 2-4 hours to obtain a nano photocatalyst A;
s3, mixing g-C 3 N 4 Mixing with nano photocatalyst A, grinding, and introducing H 2 S gas at H 2 And (3) vulcanizing for 10-16 h under the S atmosphere, and cooling to room temperature to obtain the nano photocatalyst.
2. The method of claim 1, wherein the nano-photocatalyst air deodorant is prepared by the following steps: the vegetable gum in the step 1 is one of guar gum, fenugreek gum and sesbania gum.
3. The method for preparing the nano photocatalyst air deodorant according to claim 1, wherein the nano photocatalyst in the step 1 is prepared by the following steps in parts by weight:
s1, dissolving 20-40 parts of cane sugar in 140-180 parts of water, and adding 2.4-7.4 parts of SnCl 4 ·5H 2 O, stirring for 10-20 minutes at 300-600 revolutions per minute to obtain a mixed solution; adding a sodium hydroxide aqueous solution with the concentration of 0.5-1.2 mol/L to adjust the pH value of the mixed solution to 11-13, continuously stirring for 10-30 minutes at 300-600 revolutions/minute, carrying out hydrothermal reaction in a reaction kettle, naturally cooling to 20-30 ℃, centrifuging at 5000-10000 revolutions/minute to collect solids, respectively washing for 2-4 times by using absolute ethyl alcohol and water, and drying for 3-6 hours at 60-90 ℃ to obtain carbon rubber balls/tin dioxide;
s2, putting 4.5-10.5 parts of tetrabutyl titanate and 1.8-4.2 parts of the carbon glue balls/tin dioxide prepared in the step S1 into 20-40 parts of absolute ethyl alcohol, performing ultrasonic dispersion for 10-20 minutes, and stirring for 45-90 minutes at 400-600 revolutions per minute to obtain a dispersion solution; adding 10-20 parts of tetrabutyl titanate ethanol solution with the concentration of 40-60 mg/L into the dispersion solution, and stirring for 45-90 minutes at 400-600 revolutions/minute to obtain solution A; then mixing 5-15 parts of absolute ethyl alcohol, 2-8 parts of water, 10-20 parts of acetic acid, 0.2-0.5 part of cerous nitrate hexahydrate and 0.03-0.08 part of graphene oxide, carrying out ultrasonic treatment for 2-5 minutes, and stirring for 45-90 minutes at 400-600 revolutions per minute to obtain a solution B; dropwise adding the solution B into the solution A, stirring for 4-8 hours at 400-600 revolutions per minute, carrying out hydrothermal reaction in a reaction kettle, cooling to 20-30 ℃, centrifugally collecting solids at 5000-10000 revolutions per minute, respectively cleaning for 2-4 times by using absolute ethyl alcohol and water, carrying out vacuum drying for 6-10 hours at 60-90 ℃, calcining for 2-4 hours at 650-700 ℃, and raising the temperature at 3-6 ℃/minute to obtain a nano photocatalyst A;
s3, mixing g-C 3 N 4 Mixing with the nano photocatalyst A prepared in the step S2, grinding for 10-30 minutes at 200-400 r/min, and introducing H at 15-25 mL/S 2 S gas in H 2 And vulcanizing at 178-185 ℃ for 10-16 h in S atmosphere, cooling at the rate of 10 ℃/min to 20-30 ℃ to obtain the nano photocatalyst.
4. The method for preparing a nano-photocatalyst air deodorant as claimed in claim 1 or 3, wherein: the hydrothermal reaction temperature in the step S1 and the hydrothermal reaction temperature in the step S2 are respectively 140-200 ℃, 110-150 ℃, and the hydrothermal reaction time is respectively 6-10 hours and 20-28 hours.
5. The method for preparing a nano-photocatalyst air deodorant as claimed in claim 1 or 3, wherein: g-C in said step S3 3 N 4 The weight ratio of the nano photocatalyst A prepared in the step S2 to the nano photocatalyst A is 1 (3-7).
6. The method of claim 1, wherein the nano-photocatalyst air deodorant is prepared by the following steps: the grain diameter of the ceramsite sand in the step 1 is 30-70 meshes.
7. The method of claim 1, wherein the nano-photocatalyst air deodorant is prepared by the following steps: the plant extract in the step 1 is a mixture of gardenia essential oil and honeysuckle extract according to the weight part ratio of 1 (3-10).
8. The method of claim 1, wherein the nano-photocatalyst air deodorant is prepared by the following steps: the adhesive auxiliary agent in the step 1 is a mixture of polyethylene glycol and silica sol in a weight part ratio of 1 (2-4).
9. A nano-photocatalyst air deodorant, which is characterized in that: the nano photocatalyst air deodorant is prepared by the preparation method of the nano photocatalyst air deodorant as claimed in any one of claims 1-8.
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